HPLC-MS/MS快速测定饲料中25种喹诺酮类药物

Rapid determination of 25 quinolones in feed by HPLC-MS/MS

为建立固相萃取柱结合液相色谱-串联质谱同步检测饲料中25种喹诺酮类药物的方法,本实验对提取溶剂、净化等前处理条件及LC-MS/MS分析条件进行了优化。结果表明:饲料样品经1%甲酸乙腈提取,PRiME HLB柱净化,氮吹至近干,用0.5 mL乙腈/0.1%甲酸溶液(1:9)定容后测定,回收率大于75%,标准偏差小于15%,检出限为10~50.0 ng/g。该方法准确、可靠、灵敏度高,适用于饲料中25种喹诺酮类药物的确证检测和定量分析。

To establish a method for simultaneous detection of 25 quinolones in feed by solid-phase extraction column combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS),the extraction solvent,purification and other pre-treatment conditions and LC-MS/MS analysis conditions were optimized in this experiment.The results showed that the feed samples were extracted by 1%formic acid acetonitrile,purified by prime HLB column,nitrogen blown to nearly dry,and measured with 0.5 mL of acetonitrile/0.1%formic acid solution(1:9).The recovery was more than 75%,the standard deviation was less than 15%,and the detection limit was 10~50.0 ng/g.The method was accurate,reliable and highly sensitive,and was suitable for the confirmative monitoring and quantitative analysis of 25 quinolones in feed.